CN1583671A - Method for preparing ceramic or ceramic-base composite materials - Google Patents
Method for preparing ceramic or ceramic-base composite materials Download PDFInfo
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- CN1583671A CN1583671A CN 200410027690 CN200410027690A CN1583671A CN 1583671 A CN1583671 A CN 1583671A CN 200410027690 CN200410027690 CN 200410027690 CN 200410027690 A CN200410027690 A CN 200410027690A CN 1583671 A CN1583671 A CN 1583671A
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Abstract
A process for preparing ceramics or ceramics-base composition includes such steps as putting the prefabricated body in reacting chamber, filling precursor in it, microwave heating to generate a temp gradient with the highest temp of 800-1300 deg.C, and thermodecomposing and depositing said precursor.
Description
Technical field
The present invention relates to the preparation method of a kind of preparation method of matrix material, particularly pottery or ceramic matric composite.
Background technology
At present, sintering or isothermal chemical vapor infiltration CVI technology are adopted in the preparation of high-performance ceramic and ceramic matric composite more.And in isothermal CVI, the eliminating that gaseous precursor enters precast body and waste gas is limited by gaseous diffusion and precast body perviousness, can in precast body, produce bigger gas concentration gradient, make the solid deposition preferentially occur in the precast body surface, the hole on precast body surface is sealed prematurely, influence its inner further densification.For slowing down this phenomenon, solution commonly used is to adopt low temperature, low gas concentration, but this causes sedimentation rate very slow again; Also to repeatedly interrupt deposition procedures in addition, remove the surface crust by mechanical workout, open the storage pore, continue deposition, because sedimentary overlong time, therefore the densification cycle of whole matrix material is very long, generally need one month to several months, cause the product cost very high, influenced the widespread use of ceramic matric composite, as C-base composte material.For shortening the densification time of carbon back and ceramic matric composite, improve product properties and density uniformity, in decades, various countries have successively carried out many-sided improvement to isothermal CVI technology.Comparatively common has: 1, thermal gradient CVI, No. 5411763 disclosed methods of United States Patent (USP), as when preparing carbon/carbon compound material, can improve the homogeneity of densification effectively, but because carbon/hydrogen enters precast body and still mainly relies on diffusion, gas transmission is slow, and the material densification rate improves limited; 2, isothermal pressure gradient CVI technology, No. 4142261 disclosed methods of German patent DE, because the mass transfer mode of gas changes mobile mass transfer into, improved the transmittability of gas, sedimentation rate improves greatly, can shorten the densification time to a certain extent, but still have the problem of non-uniform of densification; 3, pulse CV I technology: be deposited on cycle operation between carbon/gas pressure and the vacuum, can significantly improve the homogeneity of densification, adopt this method very high, use seldom to equipment requirements.
U.S.'s Oak Ridge National Laboratory had proposed forced-flow heat gradient chemical gaseous phase permeation method FCVI in 1984, be No. 4580524 disclosed methods of United States Patent (USP), at first in order to the preparation ceramic matric composite, the FCVI method synthesis advantage of thermal gradient CVI and isothermal pressure gradient CVI, but finish the densification process of material within a short period of time, and the product density homogeneity is preferable, is specially adapted to the moulding of thicker product.But because in FCVI technology, the heating in each zone mainly depends on conduction of heat in the precast body, influence factor is a lot, as precast body hot-face temperature, huyashi-chuuka (cold chinese-style noodles) temperature, retainer thermal conductivity, precast body density, fibre orientation, pore dimension and structure etc., gas concentration, flow velocity also have certain influence in addition.Therefore make the temperature control of deposition region in the precast body comparatively difficult, unfavorable phenomenons such as precast body huyashi-chuuka (cold chinese-style noodles) densification deficiency may occur.
In recent years, the France researchist has proposed the fast densified metallization processes RTD of a kind of liquid-phase vaporization, No. 4472454, United States Patent (USP), the main process of RTD technology is that the charcoal fiber preform be impregnated in the liquid hydrocarbon, total system is heated to boiling point, hydrocarbon gas penetrates in the precast body, to the external sediment pyrolytic carbon, can finish the densification of carbon/carbon compound material from the lining in very short time.The principle of RTD technology is after liquid hydrocarbon reaches boiling point, and constantly gasification descends the precast body surface temperature and core keeps very high-temperature, thereby realizes liquid hydrocarbon pyrolytic deposition gradually from inside to outside in the precast body.The deficiency that this method exists is that precast body must be centered around on the heating member, can only be used in hollow member, has limited the use range of this technology greatly.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing pottery or ceramic matric composite, the technical problem that solves is to make the certain thermograde of the spontaneous generation of precast body, and generation localized hyperthermia, matrix precursor is only deposited in the high-temperature zone, and deposit less or do not deposit at cold zone, control the process of densification by the attemperation gradient, make pyrolysis product in the local deposition earlier of precast body, to integral extension, realize the even compactization of pyrolysis gradually of precast body by the part.
The present invention is by the following technical solutions: a kind of method for preparing pottery or ceramic matric composite may further comprise the steps: (1) places reaction chamber with precast body, and charges into presoma; (2) adopt microwave that precast body is heated to make and produce thermograde in the precast body, the high-temperature zone temperature is controlled between 800 ℃ to 1300 ℃; (3) presoma pyrolytic deposition in precast body, thus fine and close pottery or ceramic matric composite obtained.
When the present invention adopted microwave that precast body is heated, the cold zone temperature of precast body was controlled at below 600 ℃.
Precast body of the present invention is carbon fiber block, silicon carbide fiber block or ceramic powder molding blank.
Be added with assist medium in the precast body of the present invention.
Assist medium of the present invention is carbon dust, carbon-point, carbon piece, carborundum powder, Globar or silicon carbide bulk.
Presoma of the present invention is single constituent element gaseous precursor or multicomponent gaseous state precursor.
Gaseous precursor of the present invention is the liquid alkane of carbon/hydrogen, Sweet natural gas, vaporization, the kerosene of vaporization, the diesel oil of vaporization, the trichloromethyl silane of vaporization, silane, nitrogen, hydrogen or the ammonia of vaporization.
Presoma of the present invention can also be a liquid precursor.
Liquid precursor of the present invention is to have low viscosity and certain mobile liquid alkane, aromatic liquid hydrocarbon, thermosetting resin, pitch, kerosene, diesel oil, trichloromethyl silane or silane.
The pottery or the ceramic matric composite of the present invention's preparation are block materials.
Compared with prior art, the present invention adopts the method for microwave heating, selectivity heating characteristics by microwave, and microwave is fast to rate of heating that polar material had, the non-thermal effect of the characteristics of inner heating and microwave is to the activation of substance reaction and the inducibility of process change, fiber preform is heated rapidly, makes the certain thermograde of the spontaneous generation of precast body, there is localized hyperthermia in precast body, make matrix precursor only in the high-temperature zone deposition, and deposit less or do not deposit at cold zone.Simultaneously, microwave can promote matrix precursor on the precast body fiber pyrolytic reaction to take place, reduce pyrolysis temperature, control the process of densification by the attemperation gradient, make pyrolysis product earlier in the local deposition earlier of precast body, along with the increase of depositing time, make deposition direction by the part to integral extension, thereby realize the even compactization of pyrolysis gradually of precast body, and shorten the preparation cycle of this matrix material greatly.
Description of drawings
Fig. 1 is an embodiment of the invention gas phase infiltration densification process setting drawing.
Fig. 2 is an embodiment of the invention liquid impregnation densification process setting drawing.
Fig. 3 is precast body () sectional view that the embodiment of the invention adds assist medium.
Fig. 4 is precast body (two) sectional view that the embodiment of the invention adds assist medium.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Thinking of the present invention: the characteristics of, inner heating fast to rate of heating that polar material had according to microwave and the non-thermal effect of microwave are heated precast body rapidly to the activation of substance reaction and the inducibility of process change.Temperature is the important technical parameter in pottery or the ceramic matric composite densification process, and the carrying out of material even compactization and the weave construction of matrix are all had the significant effects effect, so temperature control is the key factor of densification.Characteristics of the present invention are in the microwave-heating densification process, utilize the characteristics of microwave rapid heating and penetrance heating, make precast body be heated to certain temperature and the certain thermograde of spontaneous formation.In the pyrolytic reaction process, because precast body local temperature height, presoma is earlier at local pyrolytic deposition, and low-temperature region is pyrolysis or not pyrolysis basically seldom, thereby the densification process of control precast body makes precast body even compactization progressively from the part to integral body.Simultaneously, along with the carrying out of reaction, presoma makes presoma have certain concentration gradient in precast body in the consumption of conversion zone, has accelerated the rate of mass transfer of presoma.Precursor flows is carried out heat exchange when precast body, the precast body surface temperature is reduced, thereby strengthens the thermograde of precast body, and along with the carrying out of reaction, gradient magnitude is tending towards a certain stationary value.Arrive the high-temperature zone of precast body when presoma after, be subjected to temperature action generation pyrolytic reaction, and be deposited on the fiber of precast body, and the prefabricated intravital hole of filling progressively, and at this moment at the low-temperature region of precast body, because temperature is low, pyrolytic reaction does not take place in presoma basically, pore channel can be not blocked, makes forerunner's physical efficiency more successfully be transferred to the pyrolysis zone of precast body.Simultaneously, microwave can promote matrix precursor on the precast body fiber pyrolytic reaction to take place, and reduces pyrolysis temperature.Carrying out in the process of deposition reaction, can control the process of densification by the attemperation gradient, make pyrolysis product earlier in the local deposition earlier of precast body, increase along with depositing time, make deposition direction by the part to integral extension, thereby realize the even compactization of pyrolysis gradually of precast body, finally finish the even compactization of whole precast body.
Precast body adopts carbon fiber block, silicon carbide fiber block or ceramic powder molding blank.
In the densification process of pottery and ceramic matric composite, the range of choice of presoma is very widely, can be single constituent element gaseous precursor or multicomponent gaseous state precursor.Gaseous precursor is the liquid alkane of carbon/hydrogen, Sweet natural gas, vaporization, the kerosene of vaporization, the diesel oil of vaporization, the trichloromethyl silane of vaporization, silane, nitrogen, hydrogen or the ammonia of vaporization.Liquid precursor is to have low viscosity and certain mobile liquid alkane, aromatic liquid hydrocarbon, thermosetting resin, pitch, kerosene, diesel oil, trichloromethyl silane or silane.
The present invention also can control, regulate the effect of microwave heating, the position of high temperature heating region and the size of thermograde by add assist medium in precast body, and cooperation matrix precursor, comprise flowing of liquid and gas, make presoma at localized high temperature regions elder generation pyrolytic deposition, and deposit less or do not deposit at cold zone, thereby the process of control densification makes pyrolysis product in the local deposition earlier of precast body, to integral extension, realize the even compactization of pyrolysis gradually of precast body by the part.Assist medium of the present invention is carbon dust, carbon-point, carbon piece, carborundum powder, Globar or silicon carbide bulk.
Embodiment 1
As shown in Figure 1, the carbon felt precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, propylene gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 800 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 2
As shown in Figure 1, the cloth lamination precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, propylene gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 3
As shown in Figure 1, carbon fiber knit body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, propylene gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 4
As shown in Figure 1, the carbon felt precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, methane gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 800 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 5
As shown in Figure 1, the cloth lamination precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, methane gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 6
As shown in Figure 1, carbon fiber knit body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, methane gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 7
As shown in Figure 1, the carbon felt precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, Sweet natural gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 800 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 8
As shown in Figure 1, the cloth lamination precast body sample 7 of reserving type is placed microwave oven heating cavity precursor reactant device ceramic shield 2, Sweet natural gas is as the gaseous precursor of RESEARCH OF PYROCARBON, with nitrogen as carrier gas and thinner, their mixed gas is fed from inlet mouth 4, employing is positioned at microwave source 5 heating of upper and lower part, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 9
As shown in Figure 1, carbon fiber knit body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, Sweet natural gas feeds from inlet mouth 4 as the gaseous precursor of RESEARCH OF PYROCARBON, employing is positioned at microwave source 5 heating of upper and lower part, and heating reaches the presoma pyrolysis temperature, and high-temperature area maintains 1100 ℃, the cold zone temperature is controlled at below 600 ℃, densification through 50 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 10
As shown in Figure 2, with kerosene as the carbon source presoma, the carbon felt precast body 7 of reserving type be impregnated in the liquid kerosene 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 800 ℃, the cold zone temperature is controlled at below 600 ℃, and kerosene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 11
As shown in Figure 2, with kerosene as the carbon source presoma, the cloth lamination precast body 7 of reserving type be impregnated in the liquid kerosene 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and kerosene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 12
As shown in Figure 2, with kerosene as the carbon source presoma, carbon fiber knit body 7 be impregnated in the liquid kerosene 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and kerosene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 13
As shown in Figure 2, with cyclohexane give is the carbon source presoma, the carbon felt precast body 7 of reserving type be impregnated in the hexanaphthene 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 800 ℃, the cold zone temperature is controlled at below 600 ℃, and hexanaphthene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 14
As shown in Figure 2, with cyclohexane give is the carbon source presoma, the cloth lamination precast body 7 of reserving type be impregnated in the hexanaphthene 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and hexanaphthene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 15
As shown in Figure 2, with cyclohexane give is the carbon source presoma, carbon fiber knit body 7 be impregnated in the liquid cyclohexane 11, and place the microwave oven heating cavity body, microwave source 5 heating around employing is positioned at, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and hexanaphthene penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 16
As shown in Figure 2, with diesel oil as the carbon source presoma, the carbon felt precast body 7 of reserving type be impregnated in the liquid diesel oil 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 800 ℃, the cold zone temperature is controlled at below 600 ℃, and diesel oil penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 17
As shown in Figure 2, with diesel oil as the carbon source presoma, the cloth lamination precast body 7 of reserving type be impregnated in the liquid diesel oil 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and diesel oil penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 18
As shown in Figure 2, with diesel oil as the carbon source presoma, carbon fiber knit body 7 be impregnated in the liquid diesel oil 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1100 ℃, the cold zone temperature is controlled at below 600 ℃, and diesel oil penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 19
As shown in Figure 3, carbon dust 12 is placed precast body 7 moulding, then, as shown in Figure 1, precast body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, adopt the gaseous precursor of propylene gas as RESEARCH OF PYROCARBON,, as carrier gas and thinner their mixed gas is fed from inlet mouth 4 with nitrogen, adopt microwave heating, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 800 ℃, and the cold zone temperature is controlled at below 600 ℃, the densification through 50 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 20
As shown in Figure 3, silicon carbide 12 is placed precast body 7 moulding, then, as shown in Figure 1, precast body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, adopt the gaseous precursor of methane as RESEARCH OF PYROCARBON,, as carrier gas and thinner their mixed gas is fed from inlet mouth 4 with nitrogen, adopt microwave heating, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, and the cold zone temperature is controlled at below 600 ℃, the densification through 50 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.75g/cm
3More than.
Embodiment 21
As shown in Figure 3, silicon carbide 12 is placed precast body 7 moulding, then, as shown in Figure 1, precast body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, adopt the gaseous precursor of Sweet natural gas as RESEARCH OF PYROCARBON,, as carrier gas and thinner their mixed gas is fed from inlet mouth 4 with nitrogen, adopt microwave heating, heating reaches the presoma pyrolysis temperature, high-temperature area maintains 1100 ℃, and the cold zone temperature is controlled at below 600 ℃, the densification through 50 hours, can finish the quick preparation of carbon/carbon compound material, last sample density is from 0.40g/cm
3Be increased to 1.75g/cm
3More than.
Embodiment 22
As shown in Figure 3, carbon piece 12 is placed precast body 7 moulding, then, as shown in Figure 2, with kerosene as the carbon source presoma, the precast body 7 of moulding be impregnated in the liquid kerosene 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, and rapid heating makes the precast body high-temperature area maintain 800 ℃, and the cold zone temperature is controlled at below 600 ℃, kerosene penetrates into vaporization and pyrolytic deposition in the precast body, densification through 30 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.65g/cm
3More than.
Embodiment 23
As shown in Figure 3, carbon piece 12 is placed precast body 7 moulding, then, as shown in Figure 2, with diesel oil as the carbon source presoma, the precast body 7 of moulding be impregnated in the liquid diesel oil 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, and rapid heating makes the precast body high-temperature area maintain 1100 ℃, and the cold zone temperature is controlled at below 600 ℃, diesel oil penetrates into vaporization and pyrolytic deposition in the precast body, densification through 30 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 24
As shown in Figure 3, silicon carbide 12 is placed precast body 7 moulding, then, as shown in Figure 2, with cyclohexane give is the carbon source presoma, the precast body 7 of moulding be impregnated in the hexanaphthene 11, and place the microwave oven heating cavity body, adopt microwave heating, because the existence of thermograde, the precast body part is by rapid heating, and rapid heating makes the precast body high-temperature area maintain 1100 ℃, and the cold zone temperature is controlled at below 600 ℃, hexanaphthene penetrates into vaporization and pyrolytic deposition in the precast body, densification through 30 hours can be finished the quick preparation of carbon/carbon compound material, and last sample density is from 0.40g/cm
3Be increased to 1.70g/cm
3More than.
Embodiment 25
As shown in Figure 1, carbon felt precast body 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, with hydrogen as carrier gas, adopt microwave heating, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, the densification through 50 hours can be finished the quick preparation of SiC based composites.Last sample density is from 0.40g/cm
3Be increased to 1.85g/cm
3More than.
Embodiment 26
As shown in Figure 1, cloth lamination precast body 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, with hydrogen as carrier gas, adopt microwave heating, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, the densification through 50 hours can be finished the quick preparation of SiC based composites.Last sample density is from 0.40g/cm
3Be increased to 1.85g/cm
3More than.
Embodiment 27
As shown in Figure 1, carbon fiber knit body 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, with hydrogen as carrier gas, adopt microwave heating, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, the densification through 50 hours can be finished the quick preparation of SiC based composites.Last sample density is from 0.40g/cm
3Be increased to 1.85g/cm
3More than.
Embodiment 28
As shown in Figure 3, silicon carbide 12 is placed 7 moulding of prefabricated carbon fiber body, then, as shown in Figure 1, precast body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, as carrier gas, adopt microwave heating with hydrogen, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, densification through 50 hours can be finished the quick preparation of SiC based composites.Last sample density is from 0.40g/cm
3Be increased to 1.85g/cm
3More than.
Embodiment 29
As shown in Figure 1, silicon carbide fiber precast body 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, with hydrogen as carrier gas.Adopt microwave heating, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, the densification through 50 hours can be finished the quick preparation of SiC/SiC matrix material.Last sample density can reach 2.5g/cm
3More than.
Embodiment 30
As shown in Figure 3, carbon dust 12 is placed 7 moulding of silicon carbide fiber precast body, then, as shown in Figure 1, precast body sample 7 is placed microwave oven heating cavity precursor reactant device ceramic shield 2, with the trichloromethyl silane of vaporization as the presoma of SiC matrix, as carrier gas, adopt microwave heating with hydrogen, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, densification through 50 hours can be finished the quick preparation of SiC/SiC matrix material.Last sample density can reach 2.5g/cm
3More than.
Embodiment 31
As shown in Figure 2, with trichloromethyl silane as matrix precursor, silicon carbide precast body 7 be impregnated in the liquid trichloromethyl silane 11, and place the microwave oven heating cavity body, adopt microwave heating, owing to there is thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1300 ℃, the cold zone temperature is controlled at below 600 ℃, and trichloromethyl silane penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of SiC/SiC matrix material, last sample density can reach 2.5g/cm
3More than.
Embodiment 32
As shown in Figure 3, carbon piece 12 is placed 7 moulding of silicon carbide precast body, then, as shown in Figure 2, with trichloromethyl silane as matrix precursor, the precast body 7 of moulding be impregnated in the liquid trichloromethyl silane 11, and place the microwave oven heating cavity body, adopt microwave heating, owing to there is thermograde, the precast body part is by rapid heating, high-temperature area maintains 1300 ℃, and the cold zone temperature is controlled at below 600 ℃, and trichloromethyl silane penetrates into vaporization and pyrolytic deposition in the precast body, densification through 30 hours can be finished the quick preparation of SiC/SiC matrix material.Last sample density can reach 2.5g/cm
3More than.
Embodiment 33
As shown in Figure 1, silicon carbide powder is placed microwave oven heating cavity precursor reactant device ceramic shield 2 through the porous body 7 that moulding obtains, with the trichloromethyl silane of vaporization presoma as the SiC matrix, with hydrogen as carrier gas.Adopt microwave heating, rapid heating reaches needed temperature, high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, the densification through 50 hours can be finished the quick preparation of SiC/SiC matrix material.Last sample density can reach 2.5g/cm
3More than.
Embodiment 34
As shown in Figure 2, with trichloromethyl silane as matrix precursor, silicon carbide powder be impregnated in the liquid trichloromethyl silane 11 through the porous body 7 that moulding obtains, and place the microwave oven heating cavity body, adopt microwave heating, owing to there is thermograde, the precast body part is by rapid heating, rapid heating makes the precast body high-temperature area maintain 1300 ℃, the cold zone temperature is controlled at below 600 ℃, and trichloromethyl silane penetrates into vaporization and pyrolytic deposition in the precast body, the densification through 30 hours, can finish the quick preparation of SiC/SiC matrix material, last sample density can reach 2.5g/cm
3More than.
Embodiment 35
As shown in Figure 1, silicon carbide powder is placed microwave oven heating cavity precursor reactant device ceramic shield 2 through the porous body 7 that moulding obtains, with NH
3With the vaporization silicon tetrachloride as Si
3N
4The presoma of matrix, with hydrogen as carrier gas.Adopt microwave heating, rapid heating reaches needed temperature, and high-temperature area maintains 1300 ℃, the cold zone temperature is controlled at below 600 ℃, under the control of thermograde, presoma in precast body from the part to integral body pyrolytic deposition progressively, densification through 50 hours can be finished SiC/Si
3N
4The quick preparation of matrix material.Last sample density can reach 2.5g/cm
3More than.
The present invention prepares the method for pottery or ceramic matric composite and uses the microwave-heating quick densifying, break through the restriction of existing CVI technology, means such as collection microwave rapid heating, spontaneous generation thermograde are one, realize the superposition of multiple acceleration scheme in same technology, develop the new technology of a kind of fast pyrogenation deposition preparation pottery or ceramic matric composite.The present invention adopts microwave to heat precast body, thereby prepares pottery or ceramic matric composite by the microwave rapid heating; Because microwave heating has inner heating, through heating, thus spontaneous generation thermograde, make precast body by the part to integral body even compactization progressively, avoid the phenomenon that crusts, the transmission that makes presoma smoothly and quick has been saved machining process.But also can be by in precast body, adding assist medium, thereby improve the microwave heating effect of precast body, the size of attemperation gradient, the position of control high-temperature area, the mobile precast body even compactization progressively from the part to integral body that forces that cooperates presoma.Because the self-catalysis of microwave, accelerate the rate of mass transfer of presoma, promote matrix precursor that the pyrolytic deposition reaction takes place on the precast body fiber, the reduction pyrolysis temperature, play energy-conservation, the effect that reduces cost, and shorten the densification cycle greatly.
Claims (10)
1. method for preparing pottery or ceramic matric composite, may further comprise the steps: (1) places reaction chamber with precast body, and charges into presoma; (2) adopt microwave that precast body is heated to make and produce thermograde in the precast body, the high-temperature zone temperature is controlled between 800 ℃ to 1300 ℃; (3) presoma pyrolytic deposition in precast body, thus fine and close pottery or ceramic matric composite obtained.
2. the method for preparing pottery or ceramic matric composite according to claim 1 is characterized in that: when described employing microwave heated precast body, the cold zone temperature of precast body was controlled at below 600 ℃.
3. the method for preparing pottery or ceramic matric composite according to claim 2 is characterized in that: described precast body is carbon fiber block, silicon carbide fiber block or ceramic powder molding blank.
4. the method for preparing pottery or ceramic matric composite according to claim 3 is characterized in that: be added with assist medium in the described precast body.
5. the method for preparing pottery or ceramic matric composite according to claim 4 is characterized in that: described assist medium is carbon dust, carbon-point, carbon piece, carborundum powder, Globar or silicon carbide bulk.
6. according to arbitrary described method for preparing pottery or ceramic matric composite in the claim 1 to 5, it is characterized in that: described presoma is single constituent element gaseous precursor or multicomponent gaseous state precursor.
7. the method for preparing pottery or ceramic matric composite according to claim 6 is characterized in that: described gaseous precursor is the liquid alkane of carbon/hydrogen, Sweet natural gas, vaporization, the kerosene of vaporization, the diesel oil of vaporization, the trichloromethyl silane of vaporization, silane, nitrogen, hydrogen or the ammonia of vaporization.
8. according to arbitrary described method for preparing pottery or ceramic matric composite in the claim 1 to 5, it is characterized in that: described presoma can also be a liquid precursor.
9. the method for preparing pottery or ceramic matric composite according to claim 9 is characterized in that: described liquid precursor is to have low viscosity and certain mobile liquid alkane, aromatic liquid hydrocarbon, thermosetting resin, pitch, kerosene, diesel oil, trichloromethyl silane or silane.
10. according to arbitrary described method for preparing pottery or ceramic matric composite in the claim 1 to 5, it is characterized in that: the pottery of described preparation or ceramic matric composite are block materials.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492296B (en) * | 2009-03-05 | 2012-04-25 | 厦门大学 | Microwave auxiliary thermal treatment method for ceramic fibre and thermal insulation body structure |
| CN103722784A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Preparation method of laminated hybrid composite filled with resin |
| CN106007771A (en) * | 2016-05-23 | 2016-10-12 | 深圳大学 | Method for quickly preparing rough laminar pyrolytic carbon |
| CN106966746A (en) * | 2016-06-29 | 2017-07-21 | 北京航空航天大学 | Plasma enhancing microwave-heating prepares the method and device of ceramic matric composite |
| CN109553429A (en) * | 2017-09-25 | 2019-04-02 | 通用电气公司 | The method of manufacture composite material and corresponding composite material |
| CN110357631A (en) * | 2019-08-14 | 2019-10-22 | 曾杰 | Chemical gaseous phase conversion process based on microwave treatment prepares the method and apparatus of silicon carbide components |
-
2004
- 2004-06-15 CN CN 200410027690 patent/CN1290799C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492296B (en) * | 2009-03-05 | 2012-04-25 | 厦门大学 | Microwave auxiliary thermal treatment method for ceramic fibre and thermal insulation body structure |
| CN103722784A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Preparation method of laminated hybrid composite filled with resin |
| CN103722784B (en) * | 2013-09-11 | 2016-01-20 | 太仓派欧技术咨询服务有限公司 | A kind of laminated resin fills the preparation method of hybrid composite |
| CN106007771A (en) * | 2016-05-23 | 2016-10-12 | 深圳大学 | Method for quickly preparing rough laminar pyrolytic carbon |
| CN106966746A (en) * | 2016-06-29 | 2017-07-21 | 北京航空航天大学 | Plasma enhancing microwave-heating prepares the method and device of ceramic matric composite |
| CN106966746B (en) * | 2016-06-29 | 2018-05-22 | 北京航空航天大学 | Plasma enhancing microwave-heating prepares the method and device of ceramic matric composite |
| CN109553429A (en) * | 2017-09-25 | 2019-04-02 | 通用电气公司 | The method of manufacture composite material and corresponding composite material |
| CN110357631A (en) * | 2019-08-14 | 2019-10-22 | 曾杰 | Chemical gaseous phase conversion process based on microwave treatment prepares the method and apparatus of silicon carbide components |
| CN110357631B (en) * | 2019-08-14 | 2021-09-17 | 曾杰 | Method and equipment for preparing silicon carbide component by microwave treatment-based chemical vapor conversion process |
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| CN1290799C (en) | 2006-12-20 |
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